Method for Determining 11 Perfluorinated Compounds in Quartz Sand and Soil Using Anyeep TQ9120

Per- and polyfluoroalkyl substances (PFAS) are a class of synthetic persistent organic pollutants characterized by stable carbon-fluorine bonds that resist natural degradation. They exhibit long-range transport potential and bioaccumulation tendencies. Soil and sediment serve as their primary environmental sinks, acting as key vectors for PFAS entry into ecological cycles. Their contamination levels directly impact ecosystem safety and human health, making the monitoring and control of PFAS in soil and sediment a critical focus of environmental surveillance.

This study covers sample types including soil (agricultural, industrial vicinity, urban green spaces, background areas) and sediment (riverbeds, lake bottoms, marine sediments). To standardize testing procedures and ensure data accuracy and compliance, all tests strictly follow current Chinese standards, such as T/ZJEEMA XXXX-2024 "Determination of 20 Per- and Polyfluoroalkyl Substances in Soil by Liquid Chromatography-Tandem Mass Spectrometry." This method provides a scientifically reliable technical basis for pollution surveys, risk assessments, and management of PFCs in soil and sediment. This method is adapted fromHJ 1334-2023Quantified using the internal standard method.

Instruments and Reagents

Anyeep TQ120 Ultra-High Performance Liquid Chromatography-Tandem Mass SpectrometrySystem

Methanol(MS grade, ANPEL Shanghai)

Ammonium acetate (HPLC grade,Shanghai ANPEL）

Ammonia (Analytical Reagent,Shanghai ANPEL）

Acetic Acid (Analytical Reagent,Shanghai ANPEL）

Liquid Chromatography Conditions

Mobile PhaseA: 5 mM ammonium acetate–water

Mobile Phase B: Methanol

Chromatography column: Waters ACQUITY UPLC BEH C18 1.7μm, 2.1*100 mm

Column Temperature：40 ℃

Flow rate: 0.3 mL/min

Injection volume：5 μL

Mass Spectrometry Conditions

Ionization Source： Electrospray Ionization Source (ESI)-）

Source Temperature： 550 ℃

Spray Voltage： 4500 V

air curtain： 40 psi

Mist gas： 60 psi

Auxiliary Gas： 60 psi

Crash： 10

Scan Mode：MRM

Gradient elution program

Analyte MRM Parameters

Note: * indicates the quantification ion pair.

Sample Processing

Sample ProcessingWeigh approximately 2 g of the sample (accurate to ±0.01 g) and add 20.μMix the internal standard intermediate solution with 10 mL of methanol-water mixture, vortex for 1 min, and oscillate at 300 r/min at room temperature for 2 h using an extraction device. Centrifuge for 10 min. Transfer the supernatant to another centrifuge tube, add 10 mL of methanol-water mixture to the original tube containing the sample, and repeat extraction 1 times. Combine all 2 extracts. Process the combined extract through 0.8. μAdd 80 mL of water to the filtrate from the syringe filter. Adjust the pH to 6-8 using acetic acid or ammonium hydroxide, then proceed with purification.

Activate the solid-phase extraction (SPE) cartridge sequentially with 6 mL ammonia-methanol mixture, 6 mL methanol, and 6 mL water. Pass the diluted extract through the SPE cartridge at a flow rate of 3-5 mL/min. Rinse the cartridge sequentially with 6 mL water and 8 mL ammonium acetate buffer; discard the rinse fractions. Elute the cartridge with 8 mL methanol at a flow rate of 1-3 mL/min and discard the eluate. Finally, elute the cartridge with 6 mL ammonia-methanol mixture at a flow rate of 1-3 mL/min, collecting the eluate in a centrifuge tube. Concentrate the eluate to near dryness, reconstitute with methanol to a final volume of 1 mL, and mix well before 0.22. μFilter the sample using a syringe filter into an injection vial for analysis.

Standard Curve PreparationAccurately pipette the appropriate amount of mixed standard working solution and mixed internal standard working solution, then dilute with volumetric solution to0.05 μg/L,0.1 μg/L,0.2 μg/L,0.5 μg/L, 1 μg/L, 2 μg/L, 5 μg/L, 10 μg/L, 20 μg/L, 50 μg/L、100μg/L series standard solutions for determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS).

Linear Range

Summary

This study established a UHPLC-MS/MS method using the Anyeep TQ9120 for the analysis of 11 perfluorinated compounds. Results demonstrate that the method offers excellent sensitivity, stability, and linear range, making it suitable for routine analysis and detection of perfluorinated compounds.